AS 2564—1982

Australian Standard ®
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ALUMINIUM ORES—
DETERMINATION OF ALUMINIUM,
SILICON, IRON, TITANIUM AND
PHOSPHORUS CONTENTS—
WAVELENGTH DISPERSIVE
X-RAY FLUORESCENCE
SPECTROMETRIC METHOD
 This Australian standard was prepared by Committee MN/3, Aluminium Ores. It was
approved on behalf of the Council of the Standards Association of Australia on
6 July 1982 and published on 18 October 1982.

The following interests were represented on the committee responsible for the
preparation of this standard:
CSIRO, Division of Mineral Chemistry
CSIRO, Division of Soils
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Producers of aluminium ores

Processors of aluminium ores
Producers of aluminium products

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First published . . . . . . . . . . . . . . . . . . . . . . . . 1982

This standard was issued in draft form for comment as DR 81218.

ISBN 0 7262 2676 9

 3 AS 2564—1982

PREFACE
This standard was prepared by the Association’s Committee on Aluminium Ores under
the direction of the Minerals Standards Committee. It is the first standard of its type
in which an absolute method has been prepared for the analysis of a material by X-ray
fluorescence spectrometry.
X-ray fluorescence spectrometry is in common use for in-house control of the
quality of aluminium ore. The method contained in this standard is similar to that used
in many laboratories analysing aluminium ores by X-ray fluorescence spectrometry.
The standard has been prepared to enable X-ray fluorescence methods to be specified
in contracts.
The results of the test program have shown that the X-ray fluorescence method
compares favourably with the results obtained using traditional wet chemical methods.
The committee organized an inter-laboratory test program to obtain information
on the repeatability and reproducibility of the method. The following laboratories
participated in the test program:
Analabs Pty Ltd
The Australian Mineral Development Laboratories
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Australian National University, School of Geology

The Broken Hill Proprietary Co. Ltd, Central Research Laboratories
Bureau of Mineral Resources, Geology and Geophysics
CSIRO, Division of Soils
CSR Central Laboratory
Government Chemical Laboratories, Western Australia
Macquarie University, School of Earth Sciences
Queensland Alumina Limited
SGS Australia Ltd
University of Adelaide, School of Geology
The Zinc Corporation, Limited

CONTENTS
Page
C LAUSE
1 Scope and Application . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2 Referenced Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
3 Principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
4 Reagents and Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
5 Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
6 Sampling and Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
7 Preparation of Specimens Including Loss on Fusion Determination . . . 6
8 X-ray Fluorescence Measurement of Specimens . . . . . . . . . . . . . . . . . 10
9 Preliminary Check and Calculations . . . . . . . . . . . . . . . . . . . . . . . . . 11
10 Calculation of Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
11 General Treatment of Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
12 Test Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

APPENDICES
A Preparation of a Monitor Specimen . . . . . . . . . . . . . . . . . . . . . . . . . 17
B Computer Program for Data Manipulation . . . . . . . . . . . . . . . . . . . . . 19

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 AS 2564—1982 4

STANDARDS ASSOCIATION OF AUSTRALIA

Australian Standard
ALUMINIUM ORES — DETERMINATION OF ALUMINIUM, SILICON, IRON,
TITANIUM AND PHOSPHORUS CONTENTS — WAVELENGTH DISPERSIVE
X-RAY FLUORESCENCE SPECTROMETRIC METHOD

1 SCOPE AND APPLICATION. X-ray fluorescence measurements are based on

1.1 Scope. This standard sets out a method for
the determination of the contents of aluminium, sili-
con, iron, titanium, and phosphorus (expressed as the
oxides Al 2O3, SiO 2, Fe 2O3, TiO2, and P2O5) in alumin-
ium ores by wavelength dispersive X-ray fluorescence
spectrometry. The method has been designed to cope
with the high and variable loss on ignition of
aluminium ores.
1.2 Application. The method is applicable to all
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the ‘line only’ principle. Backgrounds are not
measured on each specimen, but are determined on
several blank specimens at the line positions.
Calibration is carried out using pure chemicals.
Final results are obtained after matrix corrections for
interelement effects.
Hygroscopic moisture is determined separately
on the laboratory sample in accordance with
AS XXXX, but loss on fusion is determined as part

normal aluminium ores regardless of mineralogical
type. The concentration range covered for each of the
components is given in Table 1.
TABLE 1
RANGE OF APPLICATION OF THE METHOD
Component Concentration range
percent
Al 2O3 30—65
SiO 2 1—25
Fe 2O3 2—50
TiO2 0.5—8
P 2O 5 0.02—5
Loss on ignition 10—35
2 REFERENCED DOCUMENTS. The following
documents are referred to in this standard:
AS 2563 Wavelength Dispersive X-ray
Fluorescence Spectrometers—
Methods of Test for Determination
of Precision
AS XXXX Aluminium Ores—Determination of
Hygroscopic Moisture in Analytical
Samples—Gravimetric Method*
BS 4237 Report on Reproducibility of
Methods of Chemical Analysis Used
in the Iron and Steel Industry
ISO/DP 6137 Aluminium Ores—Methods of
Sampling
ISO/DP 6140 Aluminium Ores—Preparation of
Samples
3 PRINCIPLE. The specimen on which X-ray
fluorescence measurements are made is prepared by
incorporating the test portion of the aluminium ore
sample, via fusion, into a borate glass disc using a
quench pressing procedure. By using such a speci-
men, particle size effects, which constitute a major
problem when a compacted test portion (briquette) is
used, are eliminated.
of the preparation of the glass specimen that is used
for X-ray fluorescence analysis.
4 REAGENTS AND MATERIALS.
4.1 General. During the analysis, only reagents
of recognized high purity shall be used.
NOTE: Some reagents of sufficient purity, in particular alumin-
ium oxide, are undesirable because of their hygroscopic nature.
Select a reagent with a very low water absorption capacity.
4.2 Silicon dioxide (SiO2), nominally 99.999 per-
cent SiO2.
4.3 Aluminium oxide (Al2O 3), nominally
99.999 percent Al 2O3.
4.4 Synthetic Calibration Sample.
4.4.1 Reagents.
4.4.1.1 Silicon dioxide (SiO 2) (4.2).
4.4.1.2 Aluminium oxide (Al 2O3) (4.3).
4.4.1.3 Iron(III) oxide (Fe 2O3), nominally
99.999 percent Fe 2O3.
4.4.1.4 Titanium dioxide (TiO 2), nominally
99.999 percent TiO2.
NOTE: Phosphorus is a common impurity in TiO2 and a reagent
low in phosphorus must be selected. The selected reagent should
be checked as even nominally high purity reagents can be highly
contaminated, e.g. a 99.999 percent TiO2 grade reagent has been
found to contain about 0.5 percent P 2O5.
4.4.1.5 Ammonium dihydrogen ortho-
phosphate (NH4H 2PO4).
4.4.1.6 Calcium carbonate (CaCO3).
4.4.2 Preparation. The masses of the reagents
used in preparing the synthetic calibration sample are
given in Table 2. Prior to weighing, however, the iron
(III) oxide and titanium dioxide shall be heated at
1000°C for a minimum of 1 h, while the ammonium
dihydrogen orthophosphate and calcium carbonate
shall be dried at 105°C for a similar time. Since
aluminium oxide and silicon dioxide can retain water
at 1000°C, they shall be heated at 1200°C for a mini-
mum of 2 h. The cooling of all reagents shall be
carried out in a desiccator with self-indicating silica
gel desiccant.

* In course of preparation as DR 82025.

COPYRIGHT
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AS 2564-1982, Aluminium ores - Determination of

aluminium, silicon, iron, titanium and phosphorus
contents - Wavelength dispersive X-ray
This is a free 4 page sample. Access the full version at http://infostore.saiglobal.com.

fluorescence spectrometric method

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